反应详情

Sodium borohydride (40 g, 1.0 mol) was added portion wise to a stirred solution of o-aminoacetophenone (80 g) in methanol (800 ml) at 0°, allowing the effervescence to subside between each addition. Cooling was removed and the mixture allowed to warm to reflux temperature to complete the reaction. When cool, the solvent was evaporated and the residue partioned between dichloromethane-water. The organic solution was washed successively with water and brine, dried (anhyd. MgSO4), filtered and evaporated to a light yellow oil which crystallized from petroleum spirit (40°-60°) to give white crystals (52 g, 64%), m.p. 50°-52°.

1. additionto subside between each addition
2. temperatureCooling
3. customwas removed
4. temperatureto warm
5. temperatureto reflux temperature
6. customthe reaction
7. temperatureWhen cool
8. customthe solvent was evaporated
9. washThe organic solution was washed successively with water and brine
10. dry with materialdried (anhyd. MgSO4)
11. filtrationfiltered
12. customevaporated to a light yellow oil which
13. customcrystallized from petroleum spirit (40°-60°)